CN108947504A - Submicrometer structure ultrathin alumina ceramic substrate and preparation method - Google Patents
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Abstract
The present invention provides submicrometer structure ultrathin alumina ceramic substrate and preparation method, which is characterized in that it including the following steps: (1) preparation of slurry；(2) drying and dehydrating；(3) roughing；(4) finish rolling forms；(5) punching press；(6) dumping；(7) it is sintered.The present invention significantly improves ultrathin alumina ceramic substrate green density, in a small amount of MgO, ZrO by rolling mill practice2、Y2O3Under the action of additive, the sintering character of material is significantly improved, reduces its sintering temperature, to obtain submicrometer structure ultrathin alumina ceramic substrate.
Description
Technical field
The present invention relates to a kind of preparation methods of submicrometer structure aluminium oxide ceramics, are applied particularly to 99.6% ultra-thin oxygen
Change the preparation method of aluminium ceramic substrate.
Technical background
Aluminium oxide ceramics due to the advantages that intensity is high, thermal conductivity is good, dielectric loss is small, wave is good, in thick film circuit and
It has been widely used in thin film circuit.How mass prepare ultra-thin (0.1~0.5mm), high-intensitive (> 600MPa),
The high-quality alumina ceramic substrate that thermal conductivity is good, dielectric loss is small is a technical problem.In general, high-purity alumina ceramic exists
During atmospheric hydrogen or vacuum-sintering, since sintering temperature is greater than 1700 DEG C, crystallite dimension commonly reaches several microns or several
Ten microns cause the bending strength of material lower (300~400MPa).Therefore, submicrometer structure aluminium oxide ceramics is obtained, with
Its bending strength is improved, is a difficult point of the invention.
In the research of current submicrometer structure aluminium oxide ceramics, focus on that special sintering process uses, such as hot isostatic pressing
Sintering, discharge plasma sintering and two-stage method sintering etc..As patent CN200510115465.2 use under 200MPa pressure in
1200 DEG C burn out aluminium oxide ceramics of the crystallite dimension less than 1 μm in hot isostatic pressing 10~14 hours.Patent
CN200810062630.6, which is used, obtains crystalline substance in 1050~1450 DEG C of discharge plasma sintering process under 10~200MPa pressure
The aluminium oxide ceramics that particle size is 0.3~1 μm.Patent CN201210117622.3 using double sintering method using crystal boundary migration and
The energy difference of grain growth first activates crystal boundary migration then to cool to 1150 DEG C rapidly and keep the temperature 48 hours at 1300 DEG C and obtains
The aluminium oxide ceramics that crystallite dimension is 0.8~1.5 μm.Although special sintering technique can get submicrometer structure aluminium oxide ceramics,
And Alumina Ceramics Sintering temperature is greatly lowered, but all have the following problems: (1) equipment investment cost is high, such as heat is quiet
Press agglomerating plant and discharging plasma sintering equipment very expensive, it is difficult to realize industrialization, its serious restricted application；(2) two
Section method sintering is time-consuming too long, cannot achieve industrialized production.
In addition, the ceramic sheet of mass production 0.1~0.5mm thickness is also a technical problem.High-purity, high density,
High-strength alumina ceramics are all made of ultra-fine alumina powder, granularity generally about 100~200nm, traditional the tape casting and note
Mold forming can not prepare ultra-thin ceramic substrate.Although patent CN201010554098.7, CN201010554117.6,
A kind of calendering formation technology is described in CN201110550231.1, CN201010550220.3 prepares ultrathin alumina thin slice,
But its sintering temperature is up to 1700 DEG C, it is difficult to obtain submicrometer structure alumina ceramic substrate.
Therefore, finding a kind of new method that mass prepares submicrometer structure ultrathin alumina ceramic substrate and being one has very much
The work of meaning.
Summary of the invention
The present invention provides a kind of submicrometer structure ultrathin alumina ceramic substrate, and the purpose is to produce qualified sub-micron
Structure ultrathin alumina ceramic substrate.
The technical scheme is that
Submicrometer structure ultrathin alumina ceramic substrate, it is characterised in that: contain mass fraction are as follows: 99.6 parts of purity are
99.99% nano alumina powder, 0.05~0.15 part of MgO, 0.1~0.2 part of Y2O3, 0.1~0.2 part of ZrO2；Ceramics
Density is not less than 3.9g/cm3, for crystallite dimension between 0.5~1 μm, bending strength is greater than 600MPa.
In order to solve the industrialized production of submicrometer structure ultrathin alumina ceramic substrate, propose to aoxidize using high-purity nm
Aluminium is raw material, adds a small amount of MgO, ZrO2、Y2O3To inhibit aluminium oxide ceramics crystal grain to grow up, using film rolling forming process technology
Realize ultra-thin ceramic substrate molding, potsherd after molding in air through at 1000~1200 DEG C biscuiting removing binder after,
It moves to be sintered at 1500~1550 DEG C in atmospheric hydrogen furnace and can prepare high strength slim alumina ceramic substrate.The ceramics
Volume density reaches 3.9g/cm3, 0.5~1 μm of crystallite dimension, bending strength is greater than 600MPa.
To complete above-mentioned submicrometer structure ultrathin alumina ceramic substrate, preparation method including the following steps:
(1) preparation of slurry: by mass fraction be 99.6 parts of purity be 99.99% nano alumina powder, 0.3~1 part
Mg (NO3)2 6H2O, 0.3~0.8 part of Y (NO3)3 6H2O and 0.3~0.6 part of ZrOCl2 8H2O is put into ball mill, is added
Enter deionized water and zirconium oxide abrasive ball, using ammonium hydroxide adjust pH to 9, with finally obtain 0.05~0.15 part MgO, 0.1~
0.2 part of Y2O3, 0.1~0.2 part of ZrO2；2 parts of ammonium polyacrylate dispersants are added, ball milling is carried out, preparing solid content is 50
~60% slurry；By in the slurry after ball milling be added 20~30 parts high molecular weight polyvinyl alcohol adhesive, 1 part of oleic acid and
200 parts of deionized waters continue ball milling and obtain evenly dispersed slurry；
(2) drying and dehydrating: slurry is poured into oil bath pan, and dehydration 2~4 is small at 100~130 DEG C under stirring
When, forming moisture content is about 20~30% ceramic walks；
(3) roughing: above-mentioned ceramic walk is put between two rollers of roll forming machine, the green compact film strips formed through multiple roll compacting with
Improve film strips density and uniformity and the exclusion for being conducive to stomata；
(4) finish rolling forms: the film strips edge that roughing obtains is cut away, then gradually reduces finishing mill to the gap roller,
Roll compacting is gradually carried out to film strips to thin by thickness, to obtain ultrathin aluminium oxide ceramic products blank；
(5) punching press: punching press will be carried out on the film strips merging sheet-punching machine after finish rolling, obtains the green compact of required shape and size
Piece；
(6) dumping: above-mentioned green sheet is clipped between two porous ceramic chips and carries out biscuiting at a temperature of 1100~1200 DEG C；
(7) be sintered: by above-mentioned biscuiting piece be clipped between two high temperature molybdenum plates at 1500~1550 DEG C in a hydrogen atmosphere into
Row sintering.
For the ease of the understanding of those skilled in the art, the present invention is further illustrated.
(1) it is about α-Al between 100~200nm that high-purity alumina powder used in step (1), which is partial size,2O3, compare table
Area is about 12~20m2/g。
(2) in step (1) adhesive composition and ratio are as follows: 16 parts of high molecular weight polyvinyl alcohol, 74 parts of deionized water, glycerol
10 parts.
(3) it is 20~30% mullite plates, thickness about 2~3mm that porous ceramic chip, which is porosity, in step (6).
(4) 600 DEG C are warming up to 1 DEG C/min of rate in step (6), 2 hours are kept the temperature, then with 2 DEG C/min of speed
Rate is warming up to 1100~1200 DEG C, keeps the temperature 1 hour, finally obtains ultra-thin ceramic element so that 1~3 DEG C/min of rate is slowly cooling
Base.
(5) step (7) high temperature molybdenum plate is the alloy molybdenum plate of thickness 2mm, and ultra-thin oxygen can be achieved in high temperature sintering procedure
Change aluminium ceramic substrate and flattens work.
The invention has the advantages that
By rolling mill practice, ultrathin alumina ceramic substrate green density is significantly improved, in a small amount of MgO, ZrO2、Y2O3
Under the action of additive, the sintering character of material is significantly improved, reduces its sintering temperature, so that it is ultra-thin to obtain submicrometer structure
Alumina ceramic substrate.
Detailed description of the invention
Fig. 1 is microstructure of the obtained submicrometer structure ultrathin alumina ceramic substrate of the invention under scanning electron microscope.
Specific embodiment
Embodiment 1
(1) preparation of slurry: by the purity that mass fraction is 99.6 parts be 99.99% nano alumina powder, 0.4 part
Mg(NO3)2 6H2O, 0.45 part of Y (NO3)3 6H2O and 0.56 part of ZrOCl2 8H2O is put into ball mill, and deionized water is added
With zirconium oxide abrasive ball, pH to 9 is adjusted using ammonium hydroxide, finally to obtain 0.06 part of MgO, 0.14 part of Y2O3, 0.2 part
ZrO2, 2 parts of ammonium polyacrylate dispersants are added, ball milling is carried out and prepares the slurry that solid content is 50~60%；After ball milling
20~30 parts of high molecular weight polyvinyl alcohol adhesive, 1 part of oleic acid and 200 parts of deionized waters are added in slurry, continues ball milling and obtains
Obtain evenly dispersed slurry；
(2) drying and dehydrating: slurry is poured into oil bath pan, and dehydration 2~4 is small at 100~130 DEG C under stirring
When, forming moisture content is about 20~30% ceramic walks；
(3) roughing: above-mentioned ceramic walk is put between two rollers of roll forming machine, is formed after multiple roll compacting certain thickness
Green compact film strips；To improve film strips density and uniformity and be conducive to the exclusion of stomata；
(4) finish rolling forms: the film strips edge that roughing obtains is cut away, then gradually reduces finishing mill to the gap roller,
Roll compacting is gradually carried out to film strips to thin by thickness, to obtain ultrathin aluminium oxide ceramic products blank；
(5) punching press: punching press will be carried out on the film strips merging sheet-punching machine after finish rolling, obtains the green compact of required shape and size
Piece；In favor of large-scale production and product outline size consistency；
(6) dumping: above-mentioned green sheet is clipped between two porous ceramic chips and carries out biscuiting at a temperature of 1100~1200 DEG C；
(7) be sintered: by above-mentioned biscuiting piece be clipped between two high temperature molybdenum plates at 1500~1550 DEG C in a hydrogen atmosphere into
Row sintering.
Embodiment 2
(1) preparation of slurry: by by mass fraction be 99.6 parts of purity be 99.99% nano alumina powder, 0.6 part
Mg(NO3)2 6H2O, 0.35 part of Y (NO3)3 6H2O and 0.56 part of ZrOCl2 8H2O is put into ball mill, and deionized water is added
With zirconium oxide abrasive ball, pH to 9 is adjusted using ammonium hydroxide, finally to obtain 0.1 part of MgO, 0.1 part of Y2O3, 0.2 part of ZrO2,
2 parts of ammonium polyacrylate dispersants are added, are carried out ball milling 24 hours, the slurry that solid content is 50~60% is prepared；After ball milling
Slurry in 20~30 parts of high molecular weight polyvinyl alcohol adhesive, 1 part of oleic acid and 200 parts of deionized waters are added, continue ball milling
Obtain evenly dispersed slurry；
(2) drying and dehydrating: slurry is poured into oil bath pan, and dehydration 2~4 is small at 100~130 DEG C under stirring
When, forming moisture content is about 20~30% ceramic walks；
(3) roughing: above-mentioned ceramic walk is put between two rollers of roll forming machine, the green compact film strips formed through multiple roll compacting with
Improve film strips density and uniformity and the exclusion for being conducive to stomata；
(4) finish rolling forms: the film strips edge that roughing obtains is cut away, then gradually reduces finishing mill to the gap roller,
Roll compacting is gradually carried out to film strips to thin by thickness, to obtain ultrathin aluminium oxide ceramic products blank；
(5) punching press: punching press will be carried out on the film strips merging sheet-punching machine after finish rolling, obtains the green compact of required shape and size
Piece；In favor of large-scale production and product outline size consistency；
(6) dumping: above-mentioned green sheet is clipped between two porous ceramic chips and carries out biscuiting at a temperature of 1100~1200 DEG C；
(7) be sintered: by above-mentioned biscuiting piece be clipped between two high temperature molybdenum plates at 1500~1550 DEG C in a hydrogen atmosphere into
Row sintering.
Embodiment 3
(1) preparation of slurry: by mass fraction be by 99.6 parts of purity be 99.99% nano alumina powder, 0.55 part
Mg (NO3)2 6H2O, 0.58 part of Y (NO3)3 6H2O and 0.41 part of ZrOCl2 8H2O is put into ball mill, and deionization is added
Water and zirconium oxide abrasive ball adjust pH to 9 using ammonium hydroxide, finally to obtain 0.08 part of MgO, 0.17 part of Y2O3, 0.15 part
ZrO2, 2 parts of ammonium polyacrylate dispersants are added, are carried out ball milling 24 hours, the slurry that solid content is 50~60% is prepared；By ball
20~30 parts of high molecular weight polyvinyl alcohol adhesive, 1 part of oleic acid and 200 parts of deionized waters are added in slurry after mill, continue
Ball milling obtains evenly dispersed slurry；
(2) drying and dehydrating: slurry is poured into oil bath pan, and dehydration 2~4 is small at 100~130 DEG C under stirring
When, forming moisture content is about 20~30% ceramic walks；
(3) roughing: above-mentioned ceramic walk is put between two rollers of roll forming machine, the green compact film strips formed through multiple roll compacting with
Improve film strips density and uniformity and the exclusion for being conducive to stomata；
(4) finish rolling forms: the film strips edge that roughing obtains is cut away, then gradually reduces finishing mill to the gap roller,
Roll compacting is gradually carried out to film strips to thin by thickness, to obtain ultrathin aluminium oxide ceramic products blank；
(5) punching press: punching press will be carried out on the film strips merging sheet-punching machine after finish rolling, obtains the green compact of required shape and size
Piece；In favor of large-scale production and product outline size consistency；
(6) dumping: above-mentioned green sheet is clipped between two porous ceramic chips and carries out biscuiting at a temperature of 1100~1200 DEG C；
(7) be sintered: by above-mentioned biscuiting piece be clipped between two high temperature molybdenum plates at 1500~1550 DEG C in a hydrogen atmosphere into
Row sintering.
Claims (3)
1. submicrometer structure ultrathin alumina ceramic substrate, it is characterised in that: contain mass fraction are as follows: 99.6 parts of purity are greater than
99.99% nano alumina powder, 0.05~0.15 part of MgO, 0.1~0.2 part of Y2O3, 0.1~0.2 part of ZrO2；Ceramics
Density is not less than 3.9g/cm3, for crystallite dimension between 0.5~1 μm, bending strength is greater than 600MPa.
2. the preparation method of submicrometer structure ultrathin alumina ceramic substrate, feature described in a kind of manufacturing claims 1 exist
In it including the following steps:
(1) preparation of slurry: by mass fraction be 99.6 parts of purity be 99.99% nano alumina powder, 0.3~1 part of Mg
(NO3)26H2O, 0.3~0.8 part of Y (NO3)36H2O and 0.3~0.6 part of ZrOCl28H2O is put into ball mill, addition go from
Sub- water and zirconium oxide abrasive ball adjust pH to 9 using ammonium hydroxide, with finally obtain 0.05~0.15 part MgO, 0.1~0.2 part
Y2O3, 0.1~0.2 part of ZrO2；2 parts of ammonium polyacrylate dispersants are added, ball milling is carried out, preparing solid content is 50~60%
Slurry；The high molecular weight polyvinyl alcohol adhesive, 1 part of oleic acid of 20~30 parts of addition in slurry after ball milling and 200 parts are gone
Ionized water continues ball milling and obtains evenly dispersed slurry；
(2) drying and dehydrating: slurry is poured into oil bath pan, is dehydrated 2~4 hours at 100~130 DEG C under stirring, shape
It is about 20~30% ceramic walks at moisture content；
(3) roughing: above-mentioned ceramic walk is put between two rollers of roll forming machine, forms the green compact of about 1mm thickness after multiple roll compacting
Film strips；
(4) finish rolling forms: the film strips edge that roughing obtains being cut away, then gradually reduces finishing mill between the gap roller, by thickness
Roll compacting, raising film strips relative density to 50~55% are gradually carried out to film strips to thin, and obtain the ultra-thin of 0.2~0.6mm thickness
Type aluminium oxide ceramic products blank；
(5) punching press: punching press will be carried out on the film strips merging sheet-punching machine after finish rolling, obtains the green sheet of required shape and size；With
Conducive to large-scale production and product outline size consistency；
(6) dumping: above-mentioned green sheet is clipped between two porous ceramic chips and carries out biscuiting at a temperature of 1100~1200 DEG C；
(7) it is sintered: above-mentioned biscuiting piece being clipped between two high temperature molybdenum plates and is burnt in a hydrogen atmosphere at 1500~1550 DEG C
Knot.
3. submicrometer structure ultrathin alumina ceramic substrate according to claim 2, it is characterised in that: in the step 2
The Al used2O3Powder purity is greater than 99.99%, and grain diameter is 100~200nm, and specific surface area is 12~20m2/g。
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Cited By (5)
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| CN110022622A (en) * | 2019-05-16 | 2019-07-16 | 厦门蜂涛陶瓷有限公司 | A kind of cellular alumina ceramic heating element and preparation method thereof |
| CN110436897A (en) * | 2019-09-04 | 2019-11-12 | 福建华清电子材料科技有限公司 | A kind of preparation method of ultrathin alumina ceramic substrate |
| CN111004020A (en) * | 2019-12-26 | 2020-04-14 | 淄博奥诺新材料科技有限公司 | Method for preparing high-purity alumina ceramic substrate at low temperature |
| CN114394825A (en) * | 2021-12-22 | 2022-04-26 | 西北工业大学宁波研究院 | Ceramic material and preparation method and application thereof |
| CN116675520A (en) * | 2023-06-12 | 2023-09-01 | 陕西宝光陶瓷科技有限公司 | Preparation method of 7-13um particle size calcined alpha alumina powder and high-density ceramic |
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| CN110022622A (en) * | 2019-05-16 | 2019-07-16 | 厦门蜂涛陶瓷有限公司 | A kind of cellular alumina ceramic heating element and preparation method thereof |
| CN110436897A (en) * | 2019-09-04 | 2019-11-12 | 福建华清电子材料科技有限公司 | A kind of preparation method of ultrathin alumina ceramic substrate |
| CN111004020A (en) * | 2019-12-26 | 2020-04-14 | 淄博奥诺新材料科技有限公司 | Method for preparing high-purity alumina ceramic substrate at low temperature |
| CN114394825A (en) * | 2021-12-22 | 2022-04-26 | 西北工业大学宁波研究院 | Ceramic material and preparation method and application thereof |
| CN114394825B (en) * | 2021-12-22 | 2023-10-31 | 西北工业大学宁波研究院 | Ceramic material and preparation method and application thereof |
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